HRID1845030

反应详情

EQUATION

反应方程式

HRID 1845030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a stirring solution 0.5 g (2.4 mmol) of 6-bromo-pyridine-2-carboxylic acid, 0.05 g (0.07 mmol) of dichlorobis(triphenylphosphine)-palladium(II), and 0.015 g (0.07 mmol) of copper (I) iodide in 10 mL of NEt3, 9.9 mL of 2 N Na2CO3 solution was added 0.38 g (3.7 mmol) of phenyl acetylene under nitrogen. After 12 h reflux under nitrogen, the reaction mixture was cooled and filtered. The filtrate was acidified using 2 N HCl (pH=5), and the resulting white precipitate was filtered, washed with water and dried to afford 0.5 g (51%) of 6-phenylethynyl-pyridine-2-carboxylic acid. LCMS: 224 (M+1)+.

WORKUP

后处理

  1. temperatureAfter 12 h reflux under nitrogen
  2. temperaturethe reaction mixture was cooled
  3. filtrationfiltered
  4. filtrationthe resulting white precipitate was filtered
  5. washwashed with water
  6. customdried